場放大樣品堆積毛細電泳電灑法質譜於分析乙型受體素類之開發與應用

Development and Application for the Analysis of β2-agonists by FASS-CE/ESI-MS

余逸萍(Yi-Ping Yu)

指導教授 ： 何國榮

國立臺灣大學/理學院/化學研究所/碩士(2014年)

https://doi.org/10.6342/NTU.2014.10373

摘要

毛細管電泳為簡單、高選擇性、低成本、分離效率高及分離快速的一項微量分析技術，至今廣泛應用於各分析領域，如蛋白質、核酸分離等生物領域，或醫學、藥學、食品安全等。目前，分析乙型受體素的偵測方式大多以液相層析質譜法(LC-MS)為主，主要原因為豬肉檢體中殘留的乙型受體素的含量是相當微量的，而毛細管電泳受限於進樣體積而導致靈敏度較液相層析法低，因此才未被廣泛的應用於乙型受體素殘留量的檢測。

本研究利用毛細電泳電灑法質譜結合線上濃縮技術-場放大樣品堆積法(FASS)並以選擇離子反應模式(SRM)進行掃描以提高靈敏度，並期望以毛細電泳擁有的高理論板數特性達到優異的分離效果。本研究所使用的介面為先前實驗室已開發的低流速鞘流介面銜接毛細管電泳電灑法質譜來分析豬肉樣品中17種乙型受體素。在FASS的操作下，以電動注入相較於未操作在FASS下訊號提升160到800倍。回收率範圍落於68 – 114 %間，而相對標準誤差的範圍落在4 – 19 %。其中12種乙型受體素的方法偵測極限落在30 ng/kg。

關鍵字

毛細管電泳 ； 電灑法質譜 ； 乙型受體素類 ； 場放大樣品堆積法

並列摘要

Capillary electrophoresis has an advantage that is simple, highly selective and low-cost, as well as high separation efficiency and rapid separation. Therefore CE is widely applied in various field of analysis nowadays, such as biological、food safety and so on. Due to the limitation of injection volume and thus lower sensitivity in CE, the analysis of β2-agonists is mostly performed using liquid chromatography mass spectrometry (LC-MS).

To improved tne sensitivity of CE in the analyte of β2-agonists, an on-line preconcentration technique- field amplified sample stacking (FASS) was adapted in this study . A low flow interface which was developed in our laboratory previously was used in the analysis 17 β2-agonists in the pork sample. With FASS, electrokinetic injection was selected as the injection technique, the signal enhancement was in the range of 160-800 fold. The recoveries of spiked meat sample is in the range of 68 – 114 %, and the relative standard deviations were in the range of 4 - 19 %. The method detection limit was 30 ng/kg for 12 β2-agonists.

並列關鍵字

capillary electrophoresis ； electrospray ionization mass spectrometry ； β2-agonists ； field amplified sample stacking (FASS)

參考文獻

56.行政院衛生署藥物食品檢驗局。2009。市售畜禽產品中動物用藥乙型受體素類（β-Agonists）殘留量調查。調查研究年報。第27期 188頁.

3.Polettini, A. J. Chromatogr. B 1996, 687, 27.

8.Ding, Y.; Qi, Y.; Suo, X. Anal. Methods 2013, 5, 2623.

14.Li, S.; Wang, J.; Zhao, S. J. Chromatogr. B. 2009, 877, 155.

15.Wang, W.; Zhang, Y.; Wang, J.; Shi, X.; Ye, J. Meat Sci. 2010, 85, 302.